反应详情

To a solution of 4-tert-butyl-N-(4-chloro-2-isonicotinoylphenyl)benzenesulfonamide (191 g) in dichloromethane (3000 mL) was added m-chloroperbenzoic acid (65%, 146 g) at 0° C., and the mixture was stirred for 30 min. The mixture was warmed to room temperature and stirred for 16 hr. The mixture was cooled to 0° C., 10% aqueous sodium dithionite solution (630 mL) was added, and the mixture was stirred for 30 min and extracted with chloroform. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution (500 mL) and saturated brine (500 mL). The organic layer was dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and purified by silica gel column chromatography (NH, chloroform) to give the object 4-tert-butyl-N-[4-chloro-2-(1-oxidoisonicotinoyl)phenyl]benzenesulfonamide (181 g, pale-yellow solid).

1. stirringstirred for 16 hr
2. temperatureThe mixture was cooled to 0° C.
3. stirringthe mixture was stirred for 30 min
4. extractionextracted with chloroform
5. washThe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution (500 mL) and saturated brine (500 mL)
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. customThe solvent was evaporated under reduced pressure
8. custompurified by silica gel column chromatography (NH, chloroform)